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目的采用顶空毛细管气相色谱法(HSp-CGC)测定热不稳定铵盐化合物XY03中的游离正丁胺。方法色谱柱为SE-54(50 m×0.25μm,1μm)石英毛细管柱,载气为N2(3 mL.min-1)、H2(42 mL.min-1)、空气(80 mL.min-1),检测器为FID,柱温120℃,进样温度200℃,检测温度200℃,顶空温度40℃,平衡时间90 min,进样气体1 mL。结果 1.0～10 mg.mL-1正丁胺与峰高的线性关系良好,回归方程为:Y=11.982X-9.029×103(r=0.9991),检测限为2.5 ng.mL-1(S/N≥3),定量限为10 ng.mL-1(S/N≥10);进样精密度、重复性、中间精密度(RSD)分别为2.84%、2.57%、2.35%,平均回收率为101.2%(RSD=2.07%)。3批XY03铵盐产品中游离正丁胺的含量分别为1.74%、1.73%、1.63%。结论 HSp-CGC法可选择性地将热不稳定铵盐XY03中的游离正丁胺汽化并测定,所用方法快速、简便、准确,是检测铵盐类化合物中游离胺的一种较实用的方法。
OBJECTIVE To determine free n-butylamine in thermostable ammonium compound XY03 by headspace capillary gas chromatography (HSp-CGC). Methods The column was a SE-54 (50 m × 0.25 μm, 1 μm) quartz capillary column. The carrier gas was N2 (3 mL.min-1), H2 1), the detector was FID, the column temperature was 120 ℃, the injection temperature was 200 ℃, the detection temperature was 200 ℃, the head space temperature was 40 ℃, the equilibrium time was 90 min and the sample gas was 1 mL. Results The linear relationship between 1.0 and 10 mg.mL-1 n-butylamine and peak height was good. The regression equation was Y = 11.982X-9.029 × 103 (r = 0.9991) with a detection limit of 2.5 ng.mL- N≥3), and the limit of quantification was 10 ng.mL-1 (S / N≥10). The precision, repeatability and RSD were 2.84%, 2.57% and 2.35%, respectively. The average recoveries Was 101.2% (RSD = 2.07%). The contents of free n-butylamine in three batches of XY03 ammonium salt products were 1.74%, 1.73% and 1.63% respectively. Conclusion The HSp-CGC method can be used to selectively vaporize free n-butylamine in the thermostable ammonium salt XY03. The method is rapid, simple and accurate and is a more practical method for the determination of free amines in ammonium salts .